HRID58171

反应详情

EQUATION

反应方程式

HRID 58171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of [2-(3-fluoro-4-nitro-phenyl)-vinyl]-dimethyl-amine (1.7 g, 8 mmol) in MeOH, was added NaBH3CN (770 g, 12 mmol) and one drop of AcOH. The reaction mixture was stirred at room temperature for 2 hours and quenched with water. After removal of all volatiles in vacuo, the residue was extracted with 10% methanol in DCM twice. The combined extracts were washed with brine, dried over anhydrous sodium sulfate. Concentration under vacuum gave a crude product, which was purified by reverse phase column to afford the title compound (1.08 g, yield: 63%). MS (ESI): 213 [M+H]+

WORKUP

后处理

  1. customquenched with water
  2. customAfter removal of all volatiles in vacuo
  3. extractionthe residue was extracted with 10% methanol in DCM twice
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationConcentration under vacuum
  7. customgave a crude product, which
  8. customwas purified by reverse phase column